反応 #4840

反応方程式

ether

methyl 3-bromo-3-methyl-{4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]phenyl}propanoate

tetrahydrofuran

→

3-methyl-3-{4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]phenyl}-2-propenoic acid

反応条件

後処理

1. 1
   その他The resulting reaction mixture
2. 2
   その他the reaction
3. 3
   その他The solvent can be removed
4. 4
   workup.DISSOLUTIONthe residual oil dissolved in ether
5. 5
   その他to obtain an ether solution which
6. 6
   抽出can be extracted with 1N hydrochloride acid
7. 7
   温度The resulting sodium hydroxide solution can be heated on the steam bath
8. 8
   温度cooled
9. 9
   その他to obtain a product which
10. 10
    乾燥The resulting ether solution can be dried with anhydrous magnesium sulfate
11. 11
    ろ過filtered
12. 12
    その他evaporated

実験手順

To a solution of methyl 3-bromo-3-methyl-{4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]phenyl}propanoate in tetrahydrofuran can be added an equivalent amount of 1,5-diazabicyclo[3.4.0]nonene-5. The resulting reaction mixture can be stirred at elevated temperature until thin layer chromatographic analysis of a reaction sample indicates the reaction to be complete. The solvent can be removed and the residual oil dissolved in ether to obtain an ether solution which can be extracted with 1N hydrochloride acid and then by 2N sodium hydroxide solution. The resulting sodium hydroxide solution can be heated on the steam bath, cooled and made acidic with concentrated hydrochloric acid to obtain a product which can be isolated from the aqueous phase with ether. The resulting ether solution can be dried with anhydrous magnesium sulfate, filtered, and evaporated to give 3-methyl-3-{4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]phenyl}-2-propenoic acid.

出典